U.S. Pat. No. 4,565,649 to Vogel discloses methods of preparing intercalated graphite compounds wherein the graphite materials are combined with an acid halide system in an inert atmosphere. The intercalated filaments obtained are washed with distilled water and dried.
U.S. Statutory Invention Registration No. H641 to McQuillan et al disclosed a method of intercalating a metal chloride into graphite fibers by placing the fibers in a tube with the intercalant, adding chlorine gas and sealing the tube under vacuum.
U.S. Pat. No. 4,849,183 to Kuriyama discloses the use of rotatable, cylindrical reaction vessel provided with an inlet for a reaction mixture and driving means rotating the vessel around an axis.
U.S. Pat. No. 4,749,514 to Murakami et al disclosed a process for the preparation of graphite intercalation compounds wherein a graphitized film or sheet with a large surface area is placed in a reaction tube, evacuated to vacuum and heated to form an intercalated compound. See Col. 4, lines 60-63. The reference discloses a number of examples wherein the intercalant is introduced in various forms (1) the vapor phase (halogen gases-F2, Br2, IC1, IBr), (2) in the liquid phase and (3) dissolved in a solvent (e.g. metal halides).